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Synthesis method of methyl nonyl acetaldehyde

A technology for the synthesis of methylnonacetaldehyde and its synthesis method, which is applied in the field of synthesis of methylnonacetaldehyde, can solve the problems of complex steps and low reaction yield, and achieve high selectivity, high reaction selectivity and mild reaction conditions Effect

Inactive Publication Date: 2018-08-10
江苏馨瑞香料有限公司
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Problems solved by technology

Although the reaction conditions of this route are mild, the steps are complicated and the reaction yield is not high.

Method used

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  • Synthesis method of methyl nonyl acetaldehyde
  • Synthesis method of methyl nonyl acetaldehyde

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Embodiment 1

[0015] Reaction: first put 1500kg of solvent methanol into the reactor of the reaction tower, then put in 300kg of morpholine, and then put in 300kg of acetic acid. After putting in acetic acid, the reaction between morpholine and acetic acid releases heat, and the reaction kettle is turned on for stirring. Then add 1600kg of 55% formaldehyde / methanol solution, and reflux begins to appear when the temperature rises to 71°C. After 20 minutes of reflux, 4750kg of undecanal is added dropwise. The dropping time is 4.5h, and the reaction temperature is 70-78°C. After reacting for 1 hour, sampling and analysis showed that the content of undecanal was 0.32%, and the reaction ended.

[0016] Recovering methanol: raise the temperature of the reactor below 90°C, the temperature of the top of the tower is below 65°C, and control the vacuum at 0.01MPa. After recovering methanol, stir for 30 minutes, let stand for 1 hour, and then separate the water.

[0017] Water washing: washing twice, ...

Embodiment 2

[0020] Reaction: first put 1500kg of solvent methanol into the reactor of the reaction tower, then put in 300kg of morpholine, and then put in 300kg of acetic acid. After putting in acetic acid, the reaction between morpholine and acetic acid releases heat, and the reaction kettle is turned on for stirring. Then add 1600kg of 55% formaldehyde / methanol solution, and reflux begins to appear when the temperature rises to 71°C. After 20 minutes of reflux, 4750kg of undecanal is added dropwise. The dropping time is 4.5h, and the reaction temperature is 70-78°C. After reacting for 1 hour, sampling and analysis showed that the content of undecanal was 0.32%, and the reaction ended.

[0021] Recovering methanol: raise the temperature of the reactor below 90°C, the temperature of the top of the tower is below 65°C, and control the vacuum at 0.01MPa. After recovering methanol, stir for 30 minutes, let stand for 1 hour, and then separate the water.

[0022] Water washing: washing twice, ...

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Abstract

The invention provides a synthesis method of methyl nonyl acetaldehyde. The synthesis method comprises the following steps: (a) taking n-undecylic aldehyde and formaldehyde as raw materials and morpholine / acetic acid as a catalyst in a solvent; adding n-undecylic aldehyde into a reaction system in a dropwise adding manner; reacting at 70 to 80 DEG C to generate methylene undecylic aldehyde; (b) taking methylene undecylic aldehyde as a raw material and palladium / carbon as a catalyst, and carrying out hydrogenation reaction to generate methyl nonyl acetaldehyde. The synthesis method of methyl nonyl acetaldehyde has the advantages of moderate reaction conditions, high reaction selectivity and high yield.

Description

technical field [0001] The present invention relates to a kind of synthesis method of methyl nonacetaldehyde. Background technique [0002] Methyl nonacetaldehyde is an important raw material for the preparation of modern flavors, which has an aldehyde aroma accompanied by notes of ambergris, citrus and vanilla. Because of its strong aroma, good diffusivity and long-lasting fragrance, it is often used as the top fragrance of aldehyde fragrance, and it can also be used in the preparation of flavors such as tobacco flavor and amber fragrance. In addition, it can also be directly used as a raw material for cosmetics and food flavors. [0003] There are two main synthetic routes of methylnonacetaldehyde: one uses undecanal and methanol as starting materials, first reacts in an autoclave to obtain α-methyl-undecanol, and then dehydrogenates to obtain methylnonacetaldehyde aldehyde. The reaction conditions of this route are harsh, and the yield is also low. Another method uses...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/62C07C47/02
CPCC07C45/62C07C45/75C07C47/02C07C47/21
Inventor 翁卫栋席建中刘洋应思斌应登宇
Owner 江苏馨瑞香料有限公司
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